JP5660004B2 - ZnMgO膜の製造方法 - Google Patents
ZnMgO膜の製造方法 Download PDFInfo
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- 229910003363 ZnMgO Inorganic materials 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title claims description 16
- 239000011777 magnesium Substances 0.000 claims description 80
- 239000011701 zinc Substances 0.000 claims description 70
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 55
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 49
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 48
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 45
- 239000002994 raw material Substances 0.000 claims description 33
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 29
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 29
- 239000007864 aqueous solution Substances 0.000 claims description 22
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 15
- 238000010587 phase diagram Methods 0.000 claims description 10
- 238000010304 firing Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000010408 film Substances 0.000 description 40
- 238000002441 X-ray diffraction Methods 0.000 description 19
- 238000000034 method Methods 0.000 description 14
- 239000000758 substrate Substances 0.000 description 10
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 8
- 239000011654 magnesium acetate Substances 0.000 description 8
- 235000011285 magnesium acetate Nutrition 0.000 description 8
- 229940069446 magnesium acetate Drugs 0.000 description 8
- 239000012528 membrane Substances 0.000 description 6
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 230000031700 light absorption Effects 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 239000006104 solid solution Substances 0.000 description 5
- 239000004246 zinc acetate Substances 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 238000004544 sputter deposition Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000005361 soda-lime glass Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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Description
本発明の第1の態様は、亜鉛イオン濃度及びマグネシウムイオン濃度を縦軸とし且つpHを横軸とする水溶液状態図で、Zn(OH)2が析出する領域とZnO2 2−が存在し得る領域とを画定する線αが、マグネシウムイオンが存在し得る領域とMg(OH)2が析出する領域とを画定する線βよりも低pH側に位置する温度のアンモニア水溶液に、Zn原料及びMg原料を溶解し、線αと線βとで挟まれた領域となるようにアンモニア水溶液のpH並びにアンモニア水溶液中の亜鉛イオン濃度及びマグネシウムイオン濃度を調整する調整工程と、該調整工程後に、アンモニア水溶液の温度を、Zn(OH)2及びMg(OH)2が析出する温度に高める加温工程と、該加温工程後に、析出物を焼成する焼成工程と、を有する、ZnMgO膜の製造方法である。
水180ml及び10%アンモニア水5〜30mlをビーカに入れ、これを氷水に浸けてアンモニア水溶液の温度が5℃になるまで冷却した。一方、Zn原料(酢酸亜鉛)及びMg原料(酢酸マグネシウム)をモル比で酢酸亜鉛:酢酸マグネシウム=6:4、7:3、8:2、9:1、及び、1:0となるように秤量し、これを上記ビーカに入れた。そして、このビーカに回転子を入れ、スターラー上で良く攪拌させることにより、酢酸亜鉛や酢酸マグネシウムを溶解させた。なお、酢酸マグネシウムを用いなかった条件を除き、酢酸亜鉛や酢酸マグネシウムを溶解させた後のアンモニア水溶液は、線αと線βとで挟まれた領域となるように調整した。
酢酸亜鉛や酢酸マグネシウムを溶解させた後、ビーカに石英ガラス基板を投入した。そして、アンモニア水溶液を攪拌しながら、60℃に加熱したウォーターバスに上記ビーカを浸け、30分間に亘って保持した。その後、石英ガラス基板を取り出して乾燥させ、500℃で1時間に亘って大気中で焼成した。以上の工程を経ることにより、膜(酢酸マグネシウムを用いなかった条件ではZnO膜、酢酸マグネシウムを用いた条件ではZnMgO膜。以下において同じ。)を製造した。
X線回折装置(Smart−Lab、株式会社リガク製)を用いて、X線回折測定を行った。結果を図6、図7、及び、表1に示す。図6の縦軸はCounts[a.u.]、同横軸は回折角2θ[°]である。図7は、原料比Mg/(Zn+Mg)[mol%]とX線回折測定で(002)ピークが確認された回折角2θ[°]との関係を示す図である。図7の縦軸は(002)のピークが確認された回折角2θ[°]、同横軸は原料比Mg/(Zn+Mg)[mol%]である。
また、紫外可視分光光度計(V−570、日本分光株式会社製)を用いて光吸収係数を測定することにより、作製した膜のバンドギャップを特定した。バンドギャップの結果を表1、図9、及び、図10に示す。図9の縦軸は光吸収係数αの2乗[a.u.]、同横軸はエネルギーhν[eV]である。スペクトルの外挿線からバンドギャップを求めた。図10の縦軸はバンドギャップ[eV]、同横軸は原料比Mg/(Zn+Mg)[mol%]である。なお、表1における固溶Mg量[mol%]は、下記式(1)から求めた。
図6及び図7に示したように、原料のMg比率が増加すると共に、(002)回折ピークが高角側にシフトした。これは、Zn(イオン半径0.74Å)サイトにイオン半径0.65ÅのMgが置換し、C軸方向に結晶が収縮したためであると考えられる。このX線回折測定結果より、条件1〜4の膜はZnMgO膜であると判断した。
Mg固溶量[mol%] = (バンドギャップ−3.2)/0.02 …式(1)
条件1の膜のバンドギャップは3.85eVであるから、式(1)よりこの膜のMg固溶量は32.5mol%である。したがって、本発明によれば、Znに対するMg固溶量を30mol%以上にすることが可能なZnMgO膜の製造方法及びZnに対するMg添加量が30mol%以上であるZnMgO膜を提供できる。
Claims (2)
- 亜鉛イオン濃度及びマグネシウムイオン濃度を縦軸とし且つpHを横軸とする水溶液状態図で、Zn(OH)2が析出する領域とZnO2 2−が存在し得る領域とを画定する線αが、マグネシウムイオンが存在し得る領域とMg(OH)2が析出する領域とを画定する線βよりも低pH側に位置する温度のアンモニア水溶液に、Zn原料及びMg原料を溶解し、前記線αと前記線βとで挟まれた領域となるように、前記アンモニア水溶液のpH並びに前記アンモニア水溶液中の亜鉛イオン濃度及びマグネシウムイオン濃度を調整する、調整工程と、
前記調整工程後に、前記アンモニア水溶液の温度を、Zn(OH)2及びMg(OH)2が析出する温度に高める、加温工程と、
前記加温工程後に、析出物を焼成する、焼成工程と、
を有する、ZnMgO膜の製造方法。 - 前記線αが前記線βよりも低pH側に位置する前記温度が25℃以下である、請求項1に記載のZnMgO膜の製造方法。
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011235630A JP5660004B2 (ja) | 2011-10-27 | 2011-10-27 | ZnMgO膜の製造方法 |
CN201280053151.2A CN103890230A (zh) | 2011-10-27 | 2012-10-25 | 制造ZnMgO膜的方法 |
PCT/IB2012/002138 WO2013061134A2 (en) | 2011-10-27 | 2012-10-25 | Znmgo film and method of manufacturing znmgo film |
EP12799592.6A EP2771498A2 (en) | 2011-10-27 | 2012-10-25 | Method of manufacturing znmgo film |
US14/354,000 US20140311564A1 (en) | 2011-10-27 | 2012-10-25 | Znmgo film and method of manufacturing znmgo film |
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JP2011235630A JP5660004B2 (ja) | 2011-10-27 | 2011-10-27 | ZnMgO膜の製造方法 |
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EP (1) | EP2771498A2 (ja) |
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JP6265362B2 (ja) * | 2012-02-27 | 2018-01-24 | 日東電工株式会社 | Cigs系化合物太陽電池 |
JP2014011310A (ja) * | 2012-06-29 | 2014-01-20 | Toyota Motor Corp | 半導体膜の製造方法 |
CN110970529A (zh) * | 2019-12-06 | 2020-04-07 | 中国科学院长春光学精密机械与物理研究所 | 一种高性能混相ZnMgO薄膜的制备方法及ZnMgO薄膜 |
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US6423983B1 (en) * | 2000-10-13 | 2002-07-23 | North Carolina State University | Optoelectronic and microelectronic devices including cubic ZnMgO and/or CdMgO alloys |
CN100342049C (zh) * | 2005-09-09 | 2007-10-10 | 浙江大学 | 立方相纳米ZnMgO线材料及其制备方法 |
CN101235537B (zh) * | 2007-11-12 | 2011-12-28 | 中国科学院长春光学精密机械与物理研究所 | 制备ZnMgO合金薄膜的方法 |
US7972899B2 (en) * | 2009-07-30 | 2011-07-05 | Sisom Thin Films Llc | Method for fabricating copper-containing ternary and quaternary chalcogenide thin films |
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CN103890230A (zh) | 2014-06-25 |
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WO2013061134A3 (en) | 2013-08-22 |
US20140311564A1 (en) | 2014-10-23 |
WO2013061134A2 (en) | 2013-05-02 |
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